Method of treating distillery-wash.



UNITED STATES PATENT OFFICE.

GEORGES MEUNIER, OF RAAB, AUSTRIA-HUNGARY, ASSIGNOR TO AUGUST LEDERERAND EMIL LEDERER, BOTH OF VIENNA, AUSTRIA-HUNGARY.

METHOD OF TREATING DISTILLERY-WASH.

momma.

No Drawing.

To all whom it may concern Be it known that I, GEoRoEs MEUNIER, a

citizen of the French Republic, residing at- Raab, in Austria-Hungary,have invented certain new and useful Improvements in Methods of TreatingDistilleryash, of which the following is a specification.

The present specification has for its object an improved method ofextracting glycerin from distillery wash. According to this method, thedistillery wash, which may be of any strength, is mixed with a specialabsorbent resulting from the carbonization by acids, either wholly orpartially, of lignocellulose according to known methods, and by way ofexample, it may be mentioned that three parts by weight of beet-rootmolasses wash at 40 B. can be absorbed by one part by weight of theabsorbent. l

The carbonization of the ligno-cellulose constituting the absorbent maybe effected either by means of free acids alone or, preferably, by meansof compounds which tend to form such acid. For instance, in order toobtain a partly carbonized ligno-cellulose freed from incrustingsubstances, 100 parts of saw-dust with about 40 parts of a dilutesolution, which contains about 1.2 parts of table salt and 1 part ofsulfuric acid at 66 B., can be intimately mixed in a wooden drum, andthe saw-dust, which has been saturated with this solution, is then driedat a temperature not exceeding 90 to 100 C., whereby, under the actionof the hydrochloric acid formed by the salt and sulfuric acid, a partialcarbonization of the lignocellulose, as well as the conversion of theincrusting substances accompanying the same into volatile organic acids,take place. Besides a certain quantity of finely powdered material,there is obtained a mass of larger particles consisting of partiallycarbonized cellulose which acts as an absorbent suitable for thedistillery wash to be treated. The absorbent contains a small quantity,(3 to 3.5%), of sodium sulfate, produced by the reaction of the sulfuricacid and the salt, which acts as a drier for the wash after itsabsorption.

If the object is to produce a wholly carbonized cellulose freed fromincrusting substances, it is advisable to treat the product obtained inthe above described manner, (2'. e., the partially carbonizedcellulose),

Specification of Letters Patent.

Patented Aug. 11, 1914:.

Application filed May 17, 1911. Serial No. 627,850.

with a mixture of salt and sulfuric acid, in which instance theproportions of the two ingredients are such as to enable them to bringabout the complete carbonizat-ion of the cellulose. For example, 100parts of partially carbonized cellulose, are intimately mixed with about40 to -15 parts of a solution which contains about 4 to 4.2 parts ofsulfuric acid at 66 B. and about 4.7 to 5 parts of table salt. Theuniformly saturated mass is then dried at from 100 to 150 C. The coarserparticles obtained, (besides a certain quantity of pulverulent carbon tobe converted into briquets), consist of wholly carbonized cellulose andcontain from 10% to 12% of sodium sulfate, and they can be employedwithout further treatment as an absorbent for the distillers washcontaining glycerin. Whether it is preferable to mix with the washpartially or wholly carbonized cellulose, or a mixture of both, dependsupon the nature of the wash to be treated, and can be easily ascertainedby preliminary trials with small quantities. For molasses wash, forinstance, a' mixture of the two absorbents above mentioned, in equalparts, has proved most advantageous.

The mixture of the absorbent wash is parts benzene, which serves toeliminate the.

greasy and resinous matters, most of the water remaining being carriedaway. Experience has shown that during this preliminary washing there isno carrying away of glycerin, but only of the water and of the solutionsof grease, resins, coloring matter and acetic or other acids, thebenzene fiowing off colorless and limpid at the comple tion of thewashing operation. The glycerin is then dissolved, the washing beingeither methodical or not, although methodical washing is moreadvantageous. The temperature of the solvent is preferably about 20 to25 C. At this temperature, in the case of molasses wash, the extractionis rapid and the product purer than at a higher temperature, a lowertemperature of the solvent conducing to a slower and less advantageousdissolution. The mixture of alcohol, benzene and glycerin resulting fromthe extraction so conducted is filtered, if necessary. Once or twice itsvolume of pure benzene is then added, the addition of this excess ofbenzene being made, preferably, while the mixture is being vigorouslycooled, thisexcess of benzene having the efiect of precipitating theglycerin contained in said mixture.

The precipitated glycerin is collected by decanting, and in order torender it purer, it may be treated in the same manner as the initialwash, or it may be distilled in a vacuum, according to known processes.The matter which remains as residue after action of the solvent andabsorbent is washed ofi by means of a saline solution, and the solventis drawn off by the said saline solution. In distilling this mixture,the solvent is collected on the one hand, and on the other hand a liquidwhich will serve as a washing liquid during a succeeding operation. Aquantity of fresh saline solution should always be added to compensatefor that which remains in the washed .mass.

The mass obtained as residue after the washing with the saline solutionconsists of the wash freed from glycerin and of the absorbent. This massis susceptible of varied uses; for instance, it may be washed. the

absorbent then recovered, and the washing liquid utilized for irrigationof land. It may also be burned under generators, the residue remainingin the form of pearl-ash. Finally, cyanogen combinations may be drawnofi' by known processes.

It follows that the above method is applicable to the extraction ofglycerin from distillery washes themselves as well as to the extractionof glycerin more or less pure from raw glycerins.

I claim The herein described method of extracting glycerin fromdistilled washes in a cold state which consists in mixing with the washan absorbent composed of acid-carbonized lignocellulose; drying themixture; washing the said mixture with a mixture of alcohol and benzene,to extract the glycerin in a cold state, and precipitating the glycerinin a cold state.

In testimony whereof I have hereunto set my hand in presence of twosubscribing witnesses.

GEORGES MEUNIER.

Witnesses:

J OSEF RUBURECHT, AUGUST Fuecnn.

